CN112174244A - Device and method for treating medium-low concentration DMF (dimethyl formamide) wastewater - Google Patents
Device and method for treating medium-low concentration DMF (dimethyl formamide) wastewater Download PDFInfo
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- CN112174244A CN112174244A CN202011026361.5A CN202011026361A CN112174244A CN 112174244 A CN112174244 A CN 112174244A CN 202011026361 A CN202011026361 A CN 202011026361A CN 112174244 A CN112174244 A CN 112174244A
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 title claims abstract description 313
- 239000002351 wastewater Substances 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 214
- 238000001179 sorption measurement Methods 0.000 claims abstract description 82
- 238000011069 regeneration method Methods 0.000 claims abstract description 42
- 239000002904 solvent Substances 0.000 claims abstract description 40
- 230000008929 regeneration Effects 0.000 claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 21
- 238000003795 desorption Methods 0.000 claims abstract description 10
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 43
- 238000010438 heat treatment Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 230000006837 decompression Effects 0.000 claims description 22
- 239000012156 elution solvent Substances 0.000 claims description 19
- 238000003860 storage Methods 0.000 claims description 18
- 238000002207 thermal evaporation Methods 0.000 claims description 18
- 238000011084 recovery Methods 0.000 claims description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- 239000003480 eluent Substances 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 3
- 229960001701 chloroform Drugs 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000005292 vacuum distillation Methods 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 10
- 238000011065 in-situ storage Methods 0.000 abstract description 6
- 238000010828 elution Methods 0.000 abstract description 3
- 238000003828 vacuum filtration Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 8
- 238000005265 energy consumption Methods 0.000 description 6
- 238000002336 sorption--desorption measurement Methods 0.000 description 6
- 238000004065 wastewater treatment Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention provides a device and a method for treating medium-low concentration DMF (dimethyl formamide) wastewater. The method uses active carbon to adsorb the DMF wastewater with medium/low concentration, reduces the DMF content and COD concentration in the wastewater, and improves the biodegradability of the wastewater; the active carbon which is saturated or is about to be saturated is desorbed and regenerated through solvent elution and high-temperature vacuum filtration, so that the in-situ regeneration of the active carbon is realized, the regeneration efficiency of the active carbon is improved, and the service life of the active carbon is prolonged; meanwhile, the adsorption and desorption solution is refined and DMF is recycled by adopting a rectifying tower, so that the resource recycling of DMF wastewater is realized.
Description
Technical Field
The invention belongs to the technical field of industrial wastewater treatment and recovery, and particularly relates to a device and a method for treating medium-low concentration DMF (dimethyl formamide) wastewater.
Background
N, N-Dimethylformamide (DMF) is an important chemical raw material and an organic solvent, has stable property and is widely applied to various chemical synthesis fields. But DMF waste water is difficult to biochemically treat and discharge up to the standard due to difficult biodegradation (B/C ═ 0.065) and biotoxicity. And the tolerance of the microorganism to the DMF content of inlet water is lower. For example, in the patent CN20151072525.1, a method for treating organic nitrogen DMF chemical wastewater, total nitrogen in water is required to be less than 200mg/L (DMF ≈ 1000ppm) in biochemical treatment of DMF wastewater, so that the concentration of DMF in biochemical treatment of DMF wastewater is too low, and the biochemical treatment can be performed only after the DMF wastewater is pretreated.
At present, the DMF wastewater treatment process mainly comprises a DMF recovery process (suitable for high-concentration DMF wastewater treatment) and a degradation removal process (suitable for low-concentration DMF wastewater treatment) which take rectification as a core. Because the boiling point of DMF is higher (152.8 ℃), the energy consumption of the rectification recovery process is larger, and the method is only suitable for the recovery treatment of DMF with high concentration. For example, in patent CN201510092727, the concentration of DMF recovered by rectification is 10-80%, and in patent CN201510724317, the concentration of DMF in DMF wastewater recovered by a waste water treatment system for recovering DMF at low cost is 15-20%.
The degradation technology is divided into biochemical degradation technology and physicochemical degradation technology (alkaline hydrolysis, acidolysis and oxidation). For example, in patent CN107055893A, the physicochemical degradation method is a method for treating low-concentration DMF wastewater, DMF is decomposed into formate and dimethylamine under the action of strong acid, dimethylamine is volatile, and dimethylamine can be taken out by air stripping or steam stripping, so as to achieve the purpose of reducing the COD concentration of DMF wastewater, but this method has a large acid consumption, and the stripped dimethylamine needs to be subjected to subsequent treatment, which is easy to cause secondary pollution.
The adsorption method is also used for treating low-concentration DMF wastewater, desorption regeneration of activated carbon is the key for treating wastewater by activated carbon, and the wastewater treated by activated carbon is difficult to be applied in a large scale if effective regeneration of activated carbon cannot be realized. The conventional activated carbon desorption regeneration methods mainly include thermal regeneration methods, biological regeneration methods, electrochemical regeneration methods, chemical elution regeneration methods, and the like, but only the thermal regeneration methods are industrially widely used at present. The thermal regeneration method includes a conventional furnace regeneration method and an electrothermal regeneration method. Wherein the combustion type regeneration furnace has higher energy consumption and lower energy utilization rate. The electrothermal regeneration method is an in-situ regeneration technology, for example, in the research of the electrothermal in-situ regeneration technology of the activated carbon in the literature, the activated carbon is carbonized for 5 minutes at the temperature of 800 ℃ under the electrothermal condition, and then is activated for 30 minutes by introducing steam to basically recover the adsorption performance of the activated carbon. Although the method can realize in-situ regeneration of the activated carbon, the method cannot be applied in a large scale due to high energy consumption.
The medicament leaching method is also suitable for the regeneration of the active carbon of the organic adsorbate with high concentration and low boiling point. The activated carbon can be regenerated by eluting the adsorption saturated activated carbon with dichloromethane during activated carbon desorption and performing air activity regeneration at 160 ℃ as described in experimental research on Dimethylformamide (DMF) wastewater treatment by a literature extraction-adsorption method. However, the method can gradually oxidize the activated carbon under the condition of high-temperature air stripping, so that the regeneration efficiency of the activated carbon is gradually reduced. Therefore, the existing activated carbon adsorption treatment method for low-concentration DMF wastewater can not effectively improve the regeneration efficiency of activated carbon, and meanwhile, the activated carbon regeneration energy consumption is high, the activated carbon circulation rate is low, and the large-scale application is difficult.
Disclosure of Invention
In order to solve the above problems, the present invention aims to provide a device and a method for treating DMF wastewater with medium and low concentration, which can reduce DMF content and COD concentration in wastewater by activated carbon adsorption treatment, thereby greatly improving biodegradability of wastewater; meanwhile, aiming at the defects of complicated regeneration process and low regeneration efficiency of the activated carbon, the method for regenerating the activated carbon in situ with low energy consumption is provided, and the regeneration efficiency of the activated carbon can be greatly improved; and the eluting solvent and DMF can be recovered by a rectifying device.
In order to achieve the above object, the technical solution of the present invention is as follows.
A device for treating medium-low concentration DMF wastewater comprises a water storage tank, an activated carbon adsorption tower, a first-stage reduced pressure rectifying tower, a second-stage reduced pressure rectifying tower, a solvent tank and a DMF recovery tank;
the water storage tank is filled with DMF wastewater to be treated, and is connected with a liquid inlet of the activated carbon adsorption tower through a first delivery pump and used for adsorbing DMF in the wastewater; one side of a liquid outlet of the active carbon adsorption tower is connected with a water outlet; the waste water adsorbed by the activated carbon adsorption tower is discharged through a water outlet;
the solvent tank is filled with an elution solvent, the solvent tank is connected with a liquid inlet of the activated carbon adsorption tower through a delivery pump II, a liquid outlet of the activated carbon adsorption tower is connected with a liquid inlet of the primary vacuum rectification tower through a vacuum condensation pump I, and a liquid outlet of the primary vacuum rectification tower is connected with the solvent tank to form a loop for eluting the adsorbed DMF and recovering the elution solvent;
the liquid outlet of the first-stage decompression rectifying tower is connected with the liquid inlet of the second-stage decompression rectifying tower through a vacuum condensation pump II, and the liquid outlet of the second-stage decompression rectifying tower is respectively connected with the DMF recycling tank and the water storage tank and used for recycling DMF.
Further, one side of the activated carbon adsorption tower is provided with a heating device, and the heating device is matched with the first vacuum condensation pump and used for carrying out suction filtration and separation on residual eluent in the activated carbon adsorption tower and recycling the eluent.
Further, the heating device comprises a controller, a heating element, a power supply, a voltmeter, and a temperature sensor;
the heating element is arranged on the outer wall of the activated carbon adsorption tower;
the power source is electrically connected with the heating element;
the voltmeter is connected with two ends of the heating element and used for detecting voltage;
one end of the temperature sensor extends into the activated carbon adsorption tower and is used for detecting the temperature;
the controller is respectively connected with the voltmeter, the power supply and the temperature sensor through signals.
A method for treating medium-low concentration DMF wastewater comprises the following steps:
s1, activated carbon adsorption stage
Conveying the DMF wastewater to be treated into an active carbon adsorption tower through a first conveying pump, and discharging the wastewater adsorbed by the active carbon through a water outlet;
s2, activated carbon desorption stage
Introducing the elution solvent in the solvent tank into an active carbon adsorption tower through a delivery pump; the desorbed eluent enters a first-stage reduced pressure rectifying tower through a first vacuum condensing pump to be rectified to elute a solvent;
the separated elution solvent enters a solvent tank, and the residual liquid enters a secondary decompression rectifying tower through a second vacuum condensation pump to be rectified into DMF; and (4) feeding the separated DMF into a DMF recovery tank, and refluxing the residual liquid to a water storage tank.
Further, the method also comprises the following steps:
s3, activated carbon regeneration stage
Closing a valve of the solvent tank, starting a power supply, adjusting voltage, electrifying and heating the activated carbon adsorption tower, and performing suction filtration on the activated carbon adsorption tower by using a vacuum condensation pump; and (3) the residual eluent which is pumped and filtered out sequentially passes through a first-stage reduced pressure rectifying tower and a second-stage reduced pressure rectifying tower, the eluting solvent and the DMF are respectively separated and recovered, and the residual liquid flows back to the water storage tank.
Further, in S1, the DMF content in the DMF wastewater to be treated is 0.2-10 wt%.
Further, in S2, the operating temperature of the first-stage vacuum rectification tower is 50-110 ℃, the operating pressure is 0.05-0.1MPa, and the reflux ratio at the top of the tower is 0.5-8;
the operation temperature of the second-stage decompression rectifying tower is 80-150 ℃, the operation pressure is 0.05-0.1MPa, and the reflux ratio at the top of the tower is 0.2-5.
Furthermore, the elution solvent in the solvent tank is any one or a mixture of more of dichloromethane, trichloromethane, carbon tetrachloride, methanol and ethanol.
Further, the operating conditions of the activated carbon desorption stage of step S2 are:
when the adsorption of the activated carbon adsorption tower is saturated or close to a saturated state, operating the step S2;
wherein the dosage of the elution solvent is 1-5 times of the total volume of the DMF wastewater to be treated.
Further, in step S3, the operation temperature of the activated carbon adsorption tower in the regeneration stage is 50-100 ℃.
The invention has the beneficial effects that:
1. the method can realize effective treatment of the DMF wastewater with medium and low concentration by adopting an activated carbon adsorption method, reduce the DMF content and the COD concentration in the wastewater and greatly improve the biodegradability of the wastewater.
And secondly, in-situ desorption regeneration is carried out on the activated carbon by adopting a solvent elution and high-temperature vacuum filtration mode, and compared with the traditional activated carbon regeneration method, the method has the advantages of low energy consumption, high regeneration efficiency, small loss of the activated carbon, recycling of the activated carbon and reduction of the use cost of the activated carbon.
The elution solvent and the DMF residual solution are recycled by a two-stage reduced pressure rectifying tower, can be recycled, has high solvent recovery rate, and realizes the resource recycling of the DMF wastewater.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus according to an embodiment of the present invention.
In the figure, 1, a water storage tank; 2. an activated carbon adsorption tower; 3. a first-stage decompression rectifying tower; 4. a second-stage decompression rectifying tower; 5. a first delivery pump; 6. a second delivery pump; 7. a first vacuum condensation pump; 8. a second vacuum condensation pump; 9. a power source; 10. a voltmeter; 11. a temperature sensor; 12. a solvent tank; 13. and a DMF recycling tank.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Fig. 1 is a schematic structural diagram of a device for treating DMF wastewater with medium and low concentration according to an embodiment of the present invention. The device comprises a water storage tank 1, an activated carbon adsorption tower 2, a first-stage decompression rectifying tower 3, a second-stage decompression rectifying tower 4, a solvent tank 12 and a DMF recycling tank 13.
The water storage tank 1 is filled with DMF wastewater to be treated, wherein the DMF wastewater is DMF wastewater with medium/low concentration. For example, the DMF wastewater to be treated has a DMF content of 0.2-10 wt%. The water storage tank 1 is connected with a liquid inlet of the activated carbon adsorption tower 2 through a first delivery pump 5 and is used for adsorbing DMF in the wastewater; one side of a liquid outlet of the active carbon adsorption tower 2 is connected with a water outlet; the waste water adsorbed by the activated carbon adsorption tower 2 is discharged through a water outlet.
The activated carbon adsorption tower is filled with activated carbon for adsorbing the DMF wastewater to be treated and reducing the DMF content and the COD concentration in the wastewater.
The solvent tank 12 is filled with an elution solvent for eluting DMF adsorbed on activated carbon. The solvent tank 12 is connected with the liquid inlet of the active carbon adsorption tower 2 through the second delivery pump 6, the liquid outlet of the active carbon adsorption tower is connected with the liquid inlet of the first-stage decompression rectifying tower 3 through the first vacuum condensation pump 7, and the liquid outlet of the first-stage decompression rectifying tower 3 is connected with the solvent tank 12 to form a loop for eluting the adsorbed DMF and recovering the eluting solvent. Of course, a control valve is arranged on the liquid outlet of the activated carbon adsorption tower 2 and used for controlling the liquid to be discharged from a water outlet or enter the first-stage decompression rectification tower 3 through a first vacuum condensation pump 7.
The liquid outlet of the first-stage decompression rectifying tower 3 is connected with the liquid inlet of the second-stage decompression rectifying tower 4 through a second vacuum condensing pump 8, and the liquid outlet of the second-stage decompression rectifying tower 4 is respectively connected with the DMF recycling tank 13 and the water storage tank 1, so that a loop is formed for recycling DMF.
Of course, in another embodiment of the present invention, a heating device is further disposed on one side of the activated carbon adsorption tower 2, and the heating device cooperates with the first vacuum condensation pump 7 to perform suction filtration separation on the residual eluent in the activated carbon adsorption tower 2 and recover the residual eluent.
That is, heat up the heating to the active carbon adsorption tower through heating device to cooperate with vacuum condensate pump 7, form high temperature vacuum environment in the active carbon adsorption tower from this, help continuing to carry out suction filtration separation with the eluate of remaining absorption on the active carbon in the active carbon adsorption tower, and then realize the regeneration treatment to the active carbon, make active carbon adsorption tower circulated use, reduce the use cost of active carbon, promote the resourceful reuse.
Specifically, the heating device comprises a controller, a heating element, a power supply 9, a voltmeter 10 and a temperature sensor 11.
The heating element is arranged on the outer wall of the activated carbon adsorption tower 2 and is used for heating the activated carbon adsorption tower; for example, the heating element may be a metal heating element or a liquid heating element, that is, an accommodating space is provided on an outer wall of the activated carbon adsorption tower, the accommodating space is filled with a heat conducting liquid, the heat conducting liquid is heated by an external heater, and the heated heat conducting liquid is guided into the accommodating space, so that the activated carbon adsorption tower is heated. Of course, the accommodating space can be filled with heat-conducting liquid and the metal heating plate can be additionally arranged, heat is conducted through the metal heating plate, and the heat-conducting liquid is heated.
The power supply 9 is electrically connected with the heating element and is used for controlling the heating element to start a heating program;
the voltmeter 10 is arranged at two ends of the heating element and used for detecting voltage, so that the adjustment of the power supply voltage is facilitated;
one end of the temperature sensor 11 extends into the activated carbon adsorption tower 2 and is used for detecting the temperature in the activated carbon adsorption tower;
the controller is respectively connected with the voltmeter 10, the power supply 9 and the temperature sensor 11 through signals.
The controller sets heating temperature and voltage, controls the heating element to start through the power supply, gradually raises the temperature in the activated carbon adsorption tower at the moment, sends temperature data to the controller through the temperature sensor, compares the temperature data with the set temperature, and continues to heat when the temperature is lower than the set temperature; when the temperature is equal to or higher than the set temperature, the heating is stopped.
A method for treating medium-low concentration DMF wastewater comprises the following steps:
s1, activated carbon adsorption stage
Conveying the DMF wastewater to be treated into an activated carbon adsorption tower 2 through a first conveying pump 5, and discharging the wastewater adsorbed by the activated carbon through a water outlet; wherein the content of DMF in the DMF wastewater to be treated is 0.2-10 wt%.
When the adsorption of the activated carbon adsorption tower is saturated or close to a saturated state, the operation of step S2 is performed.
S2, activated carbon desorption stage
Introducing the elution solvent in the solvent tank 12 into the activated carbon adsorption tower 2 through a second delivery pump 6; the desorbed eluent enters a first-stage decompression rectifying tower 3 through a first vacuum condensation pump 7 to rectify an elution solvent;
the separated elution solvent enters a solvent tank 12, and the residual liquid enters a secondary decompression rectifying tower 4 through a second vacuum condensation pump 8 to rectify DMF; the separated DMF enters a DMF recovery tank 13, and the rest solution flows back to the water storage tank 1;
wherein the operation temperature of the first-stage reduced pressure rectifying tower is 50-110 ℃, the operation pressure is 0.05-0.1MPa, and the reflux ratio at the top of the tower is 0.5-8;
the operation temperature of the second-stage decompression rectifying tower is 80-150 ℃, the operation pressure is 0.05-0.1MPa, and the reflux ratio at the top of the tower is 0.2-5.
The elution solvent in the solvent tank is any one or a mixture of more of dichloromethane, trichloromethane, carbon tetrachloride, methanol and ethanol.
Wherein the dosage of the elution solvent is 1-5 times of the total volume of the DMF wastewater to be treated.
S3, activated carbon regeneration stage
After the solvent is eluted, closing a valve of a solvent tank, stopping conveying the eluting solvent, starting a power supply 9, adjusting the voltage, electrifying and heating the activated carbon adsorption tower 2, and performing suction filtration on the activated carbon adsorption tower 2 by adopting a first vacuum condensation pump 7; the residual eluent after the pumping filtration passes through a first-stage reduced pressure rectifying tower 3 and a second-stage reduced pressure rectifying tower 4 in sequence, the eluting solvent and DMF are separated and recovered respectively, and the residual liquid flows back to the water storage tank 1.
In this embodiment, the operation temperature of the activated carbon adsorption tower in the regeneration stage is, of course, 50 to 100 ℃.
The pressure of the vacuum condensate pump is 0.05-0.1 MPa. The voltage of the voltmeter is 10-220V. The temperature of the temperature sensor is 50-100 ℃.
The DMF wastewater to be treated with different concentrations is treated according to the method, wherein the DMF content in the DMF wastewater to be treated is respectively 3 wt%, 5 wt% and 10 wt%.
Example 1
The COD concentration of the DMF wastewater is 53100mg/L, wherein the mass percent content of the DMF is 5%, and in addition, the wastewater also contains at least one of a small amount of saline-alkali, alcohols, esters or other organic matters.
After treatment by the above method:
the DMF content in the single-time adsorption effluent is 0.05 percent, and the removal rate is 99 percent; the COD concentration is 1760mg/L, and the COD removal rate is 96.7 percent.
The recovery rate of the eluting solvent recovered by rectification is 98.7 percent, and the content of DMF recovered by rectification is 98.5 percent;
the regeneration rate of the activated carbon adsorption tower after single adsorption-desorption is 99.7 percent;
then, 15 cycles of adsorption-desorption were carried out, and the regeneration rate of the activated carbon adsorption tower was found to be 97.3%.
Example 2
The COD concentration of the DMF wastewater is 126400mg/L, wherein the mass percent content of the DMF is 10%, and besides, the wastewater also contains at least one of a small amount of saline-alkali, alcohols, esters or other organic matters.
After treatment by the above method:
the DMF content of the DMF wastewater in the single adsorption effluent is 0.08 percent, and the removal rate is 99.2 percent; the COD concentration is 3520mg/L, and the COD removal rate is 97.2 percent.
The recovery rate of the eluting solvent recovered by rectification is 99.2 percent, and the content of DMF recovered by rectification is 98.9 percent;
the regeneration rate of the activated carbon adsorption tower after single adsorption-desorption is 99.4 percent;
then, 15 cycles of adsorption-desorption were carried out, and the regeneration rate of the activated carbon adsorption tower was found to be 96.5%.
Example 3
The COD concentration of the DMF wastewater is 35326mg/L, wherein the mass percent content of the DMF is 3%, and in addition, the wastewater also contains at least one of a small amount of saline-alkali, alcohols, esters or other organic matters.
After treatment by the above method:
the DMF content of the DMF wastewater at the water outlet of the single adsorption is 0.03 percent, and the removal rate is 99 percent; the COD concentration is 1760mg/L, and the COD removal rate is 96.7 percent.
The recovery rate of the eluting solvent recovered by rectification is 98.7 percent, and the content of DMF recovered by rectification is 98.5 percent;
the regeneration rate of the activated carbon adsorption tower after single adsorption-desorption is 99.4 percent;
and then, 15 times of cyclic adsorption-desorption were carried out, and the regeneration rate of the activated carbon adsorption tower was found to be 98.2%.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A device for treating DMF wastewater with medium and low concentration is characterized by comprising a water storage tank (1), an activated carbon adsorption tower (2), a primary decompression rectifying tower (3), a secondary decompression rectifying tower (4), a solvent tank (12) and a DMF recovery tank (13);
the water storage tank (1) is filled with DMF wastewater to be treated, and the water storage tank (1) is connected with a liquid inlet of the activated carbon adsorption tower (2) through a first delivery pump (5) and is used for adsorbing DMF in the wastewater; one side of a liquid outlet of the active carbon adsorption tower (2) is connected with a water outlet;
the solvent tank (12) is filled with elution solvent, the solvent tank (12) is connected with a liquid inlet of the activated carbon adsorption tower (2) through a delivery pump II (6), a liquid outlet of the activated carbon adsorption tower is connected with a liquid inlet of the primary vacuum rectification tower (3) through a vacuum condensation pump I (7), and a liquid outlet of the primary vacuum rectification tower (3) is connected with the solvent tank (12) to form a loop for eluting the adsorbed DMF and recovering the elution solvent;
the liquid outlet of the first-stage reduced pressure rectifying tower (3) is connected with the liquid inlet of the second-stage reduced pressure rectifying tower (4) through a vacuum condensing pump II (8), and the liquid outlet of the second-stage reduced pressure rectifying tower (4) is respectively connected with the DMF recovery tank (13) and the water storage tank (1) and used for recovering DMF.
2. The device for treating the DMF wastewater with the medium and low concentration according to claim 1, wherein a heating device is arranged on one side of the activated carbon adsorption tower (2), and the heating device is matched with the first vacuum condensation pump (7) and is used for performing suction filtration and separation on the residual eluent in the activated carbon adsorption tower (2) and recovering the residual eluent.
3. The apparatus for treating middle and low concentration DMF waste water according to claim 2, wherein the heating apparatus comprises a controller, a heating element, a power supply (9), a voltmeter (10) and a temperature sensor (11);
the heating element is arranged on the outer wall of the activated carbon adsorption tower (2);
the power supply (9) is electrically connected with the heating element;
the voltmeter (10) is connected with two ends of the heating element and used for detecting voltage;
one end of the temperature sensor (11) extends into the activated carbon adsorption tower (2) and is used for detecting the temperature;
the controller is respectively in signal connection with the voltmeter (10), the power supply (9) and the temperature sensor (11).
4. A method for treating DMF wastewater with medium and low concentration is characterized by comprising the following steps:
s1, activated carbon adsorption stage
Conveying the DMF wastewater to be treated into an activated carbon adsorption tower (2) through a first conveying pump (5), and discharging the wastewater adsorbed by activated carbon through a water outlet;
s2, activated carbon desorption stage
Introducing the elution solvent in the solvent tank (12) into the activated carbon adsorption tower (2) through a second delivery pump (6); the desorbed eluent enters a first-stage reduced pressure rectifying tower (3) through a vacuum condensation pump I (7) to rectify and elute the solvent;
the separated elution solvent enters a solvent tank (12), and the residual liquid enters a second-stage decompression rectifying tower (4) through a second vacuum condensation pump (8) to be rectified into DMF; the separated DMF enters a DMF recovery tank (13), and the rest liquid flows back to the water storage tank (1).
5. The method for treating medium-low concentration DMF wastewater according to claim 4, characterized by further comprising the following steps:
s3, activated carbon regeneration stage
Closing a valve of the solvent tank, starting a power supply (9), adjusting voltage, electrifying and heating the activated carbon adsorption tower (2), and performing suction filtration on the activated carbon adsorption tower (2) by adopting a first vacuum condensation pump (7); and (3) the residual eluent after pumping filtration sequentially passes through a first-stage reduced pressure rectifying tower (3) and a second-stage reduced pressure rectifying tower (4), the eluting solvent and DMF are respectively separated and recovered, and the residual liquid flows back to the water storage tank (1).
6. The method for treating DMF waste water with medium and low concentration according to claim 4, wherein in S1, the content of DMF in the DMF waste water to be treated is 0.2-10 wt%.
7. The method for treating medium-low concentration DMF wastewater according to claim 4, wherein in S2, the operating temperature of the first-stage vacuum distillation tower is 50-110 ℃, the operating pressure is 0.05-0.1MPa, and the reflux ratio at the top of the tower is 0.5-8;
the operation temperature of the second-stage decompression rectifying tower is 80-150 ℃, the operation pressure is 0.05-0.1MPa, and the reflux ratio at the top of the tower is 0.2-5.
8. The method for treating DMF waste water with medium and low concentration according to claim 4, wherein the elution solvent in the solvent tank is any one or more of dichloromethane, trichloromethane, carbon tetrachloride, methanol and ethanol.
9. The method for treating DMF wastewater with medium and low concentration according to claim 4, wherein the operating conditions of the activated carbon desorption stage of step S2 are as follows:
when the adsorption of the activated carbon adsorption tower is saturated or close to a saturated state, operating the step S2;
wherein the dosage of the elution solvent is 1-5 times of the total volume of the DMF wastewater to be treated.
10. The method for treating DMF wastewater with medium and low concentration according to claim 4, wherein in step S3, the operation temperature of the activated carbon adsorption tower in the regeneration stage is 50-100 ℃.
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